Brown sulfur dye and process of making same.



'. hitherto in the market.

UNITE STATES PATENT OFFICE.

HANS EBELING, OF BIEBRICH, GERMANY, ASSIGNOR TO KALLE AND COMPANY, OF BIEBRICH, GERMANY, A FIRM.

BROWN SULFUR DYE AND PROCESS OF MAKING SAME.

SPECIFICATION forming part Of Letters Patent No. 723,448, dated. March 24, 1903.

Application filed January 8, 1902.

To all whom it may concern:

Be it known that I, HANS EBELING, a subject of the King of Prussia, Emperor of Germany, and a resident of Biebrich, Germany, have invented certain new and useful Improvements in the Manufacture of a New Dye Containing Sulfur, of which the following is a specification.

I have discovered that the amido derivatives of metatoluylenediamin when melted with sulfur and sodium sulfid yield very valuable dyes, which dye cotton without a mordant permanent brown shades. An especially remarkable feature of these dyes is that the dyeing effected with them does not require any subsequent treatment and is distinguished by its being particularly fast against the action of light. In this respect the new dyes differ advantageously from the brown coloringmatters containing sulfur These new dyes have, further, the property of being capable of being diazotized on the fiber and developed with the usual developerssuch' as, for instance, beta-naphthol, metatoluylenediamin, or resorcinol.

In preparing the new dyes it is not necessary to introduce into the melt the readymade isolated amido derivatives of the metatoluylenediamin, as the same result can be obtained by melting those azo dyes which are obtained by the combination of metatoluylenediamin with diazo compounds of readilyvolatile amins. Such azo dyes are, for instance, anilin-azo metatoluylenediamin and anilin -disazo metatoluylenediamin. Nitro derivatives of metatoluylenediamin or polynitro derivatives of toluidin give in the sulfur melt dyes which are difierent from those hereinbefore described.

The following examples will serve to illustrate the manner in which this invention can be carried into practice:

Example 1: Eighty kilograms of sodium sulfid are dissolved in a little water and melted at from 110 to 120 centigrade with thirty kilograms of sulfur. While this melt is being Well stirred, twenty-five kilograms of triamido-toluol (CH NH NH NH 1, 2, 4, 5) are introduced into it, and the temperature is then Serial No. 88,905- (No specimens.)

raised gradually to from 200 to 220,centigrade and maintained until the melt has become dry.

Example 2: Eighty kilograms of sodium sulfid are dissolved in a little water and melted at from 110 to 120 centigrade with thirty kilograms of sulfur. While this-melt is being well stirred, thirty kilograms of anilinazo metatoluylenediamin are introduced into it, and the temperature is then raised gradually. The azo dye passes into the solution and a reaction takes place, which reaches its maximum at about 160 centigrade. The anilin then splits 0E and'a dark and smooth melt is formed. The temperature is then raised slowly to from 200 to 220 centigrade and maintained until the melt has become dry.

Example 3: Into a solution of thirty kilo-- grams of sulfur in eighty kilograms of sodium sulfid and a little water are introduced at a temperature of 100 to 110 centigrade thirty kilograms of the anilin-disazo-metatoluylenediamiu dye. The temperature is raised gradually while the mixture is being constantly stirred. At about from 150 to 160 centigrade the greater part of the 'anilin has split 0E. After the main reaction is over the melt is heated further to from 200 to 210 centigrade and this temperature maintained untihthe melt has become dry.

The dyes obtained in accordance with the hereinbefore-described invention dye cotton red-brown and are distinguished bytheir being perfectly fast against the action of soap and light. They can be diazotized on the fiber and developed with beta-naphthol,metatoluylenediamin, orresorcinol. In this manner brown shades of various tones are obtained.

The dyes dissolve very readily in water, the solution being brown, and they dissolve in concentrated sulfuric acid, the solution being dull brown. They are practically insoluble in alcohol. The color of the aqueous solution is not altered by soda-lye. When acids are added to the aqueous solution, a thick brown precipitate is formed.

Having now particularly described and ascertained the nature of this invention and in what manner the same is to be performed, I declare that what I claim is 1. The herein-described process of making substantive brown cotton dyes containing sulfur which consists in melting amide derivatives of metatoluylenediamin with sulfur and sodium sulfid at a high temperature.

2. The herein-described process of making a substantive brown cotton dye containing sulfur, which consists in melting sodium sulfid and sulfur at a temperature from 110 to 120 centigrade, introducing into this melt while being stirred amido derivatives of metatoluylenediamin and gradually raising the temperature of this melt to from 200 to 220 centigrade andmaintaining this temperature until the melt has become dry.

3. As anewarticle of manufacture,the new HANS EBELING.

Witnesses:

JEAN GRUND, IGNAZ ROSENBERG. 

